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Al2O3 nanoparticles and MCrAlY/nano-Al2O3 nanocomposite powder (M = Ni, Co, or NiCo) were produced using high-energy ball milling. The MCrAlY/nano-Al2O3 coating was deposited by selecting an optimum nanocomposite powder as feedstock for high-velocity oxy-gen fuel thermal spraying. The morphological and microstructural examinations of the Al2O3 nanoparticles and the commercial MCrAlY and MCrAlY/nano-Al2O3 nanocomposite powders were investigated using X-ray diffraction analysis, field-emission scanning electron microscopy coupled with electron dispersed spectroscopy, and transmission electron microscopy. The structural investigations and Williamson–Hall res-ults demonstrated that the ball-milled Al2O3 powder after 48 h has the smallest crystallite size and the highest amount of lattice strain among the as-received and ball-milled Al2O3 owing to its optimal nanocrystalline structure. In the case of developing MCrAlY/nano-Al2O3 nanocompos-ite powder, the particle size of the nanocomposite powders decreased with increasing mechanical-milling duration of the powder mixture.